CN112321634B - Preparation method and application of novel lead phenoxyacetate dinuclear structure complex - Google Patents
Preparation method and application of novel lead phenoxyacetate dinuclear structure complex Download PDFInfo
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- LCPDWSOZIOUXRV-UHFFFAOYSA-N phenoxyacetic acid Chemical compound OC(=O)COC1=CC=CC=C1 LCPDWSOZIOUXRV-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 229940046892 lead acetate Drugs 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 12
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 230000000171 quenching effect Effects 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 239000003814 drug Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 102000008100 Human Serum Albumin Human genes 0.000 description 20
- 108091006905 Human Serum Albumin Proteins 0.000 description 20
- 230000003993 interaction Effects 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000000862 absorption spectrum Methods 0.000 description 9
- 238000002189 fluorescence spectrum Methods 0.000 description 8
- 238000010791 quenching Methods 0.000 description 8
- 244000309466 calf Species 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 210000001541 thymus gland Anatomy 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000003446 ligand Substances 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 150000004696 coordination complex Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- -1 phenoxyacetic acid compound Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 108020003215 DNA Probes Proteins 0.000 description 1
- 239000003298 DNA probe Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- ZMMJGEGLRURXTF-UHFFFAOYSA-N ethidium bromide Chemical compound [Br-].C12=CC(N)=CC=C2C2=CC=C(N)C=C2[N+](CC)=C1C1=CC=CC=C1 ZMMJGEGLRURXTF-UHFFFAOYSA-N 0.000 description 1
- 229960005542 ethidium bromide Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
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- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/24—Lead compounds
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Abstract
The application provides a novel lead phenoxyacetate dinuclear structure complex, a preparation method and application thereof, and belongs to the technical field of medicine synthesis. The molecular formula of the complex is C 104 H 88 N 8 O 24 Pb 4 The molecular weight is 2662.58. The complex belongs to a triclinic system, P-1 space group, and the unit cell parameter is a= 12.8054 (19) nm, b= 13.1421 (19) nm and c= 17.084 (3) nm; α= 69.914 (2) °, β= 69.972 (2) °, γ= 85.241 (2) °. The preparation method of the novel lead phenoxyacetate dinuclear structure complex comprises the following steps: respectively dissolving phenoxyacetic acid, 2 '-bipyridine and lead acetate trihydrate in a solvent, dropwise adding a lead acetate solution into the phenoxyacetic acid solution under stirring, dropwise adding the 2,2' -bipyridine solution into a mixed solution under stirring, regulating the pH value with a NaOH solution, filtering, and standing at room temperature for a period of time to separate colorless transparent blocky crystals. The complex provided by the application interacts with CT-DNA and HSA, has a quenching effect on fluorescence of the CT-DNA and the HSA, and has the advantages of simple process, low cost, good repeatability, high yield and the like.
Description
Technical Field
The application relates to the technical field of medicine synthesis, in particular to a novel lead phenoxyacetate dinuclear structure complex, a preparation method and application thereof.
Background
The phenoxyacetic acid compound has strong physiological activity and is widely applied to the fields of pesticides, medicines and the like. The metal complex is formed by coordination bonds between metal ions and organic ligands, has various excellent properties, and is applied to the fields of optics, magnetism, electrochemistry, catalysis, biomedicine and the like. In recent years, the synthesis and property research of metal organic complexes have been attracting attention, for example Zheng Baohua in 2016, metal organic complexes with novel structures are constructed based on rigid polycarboxylic acid ligands and transition metal ions, and the magnetic and fluorescent properties of the metal organic complexes are studied; wang Zuopeng in 2018, synthesizing an aromatic carboxylic acid ligand and transition metal salt to obtain metal organic complexes with different dimensional space structures, and researching properties such as fluorescence and adsorption of part of the complexes; wang Xiaoting in 2019, the magnetic properties, fluorescence properties and the like of the complex were studied by using asymmetric carboxylic acid ligands and transition metals for synthesis. These findings provide a great deal of theoretical basis for the synthesis of novel metal-organic complexes.
The interaction of the complex with DNA has been an important subject of research, which has a very important role in the development of anticancer drugs and DNA probe reagents. HSA has the characteristics of small molecular weight, good stability, good water solubility, easy purification and the like, so that the HSA has high application value in the fields of pharmacology, clinical medicine, molecular biology and the like, and in addition, the HSA is a transport carrier of medicines. Therefore, by exploring the interaction between the complex and DNA and human serum albumin, the method has important significance for understanding the mechanism of the complex in vivo transportation.
Disclosure of Invention
The application aims at: aiming at the problems, the application provides a novel lead phenoxyacetate dinuclear structure complex, a preparation method and application thereof, and the application has the advantages of simple process, low cost, good repeatability, high yield and the like.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
the application firstly provides a novel lead phenoxyacetate dinuclear structure complexHas the molecular formula of C 104 H 88 N 8 O 24 Pb 4 The molecular weight is 2662.58. The complex belongs to a triclinic system, P-1 space group, and the unit cell parameter is a= 12.8054 (19) nm, b= 13.1421 (19) nm and c= 17.084 (3) nm; α= 69.914 (2) °, β= 69.972 (2) °, γ= 85.241 (2) °. The implementation formula of the complex is as follows:
the application also provides a preparation method of the novel lead phenoxyacetate dinuclear structure complex, which comprises the following steps: respectively dissolving phenoxyacetic acid, 2 '-bipyridine and lead acetate trihydrate in a solvent, dropwise adding a lead acetate solution into the phenoxyacetic acid solution under stirring, dropwise adding the 2,2' -bipyridine solution into a mixed solution under stirring, regulating the pH value with a NaOH solution, filtering, and standing at room temperature for a period of time to separate colorless transparent blocky crystals.
In the present application, it is preferable that the molar ratio of phenoxyacetic acid, 2' -bipyridine, and lead acetate trihydrate is 1:0.8-1.2:0.8-1.2.
In the present application, preferably, the pH is 6.0 to 6.5, and the standing time at room temperature is 10 to 15 days.
In the present application, preferably, the solvent is ethanol and ethanol-water mixed solvent.
In summary, due to the adoption of the technical scheme, the beneficial effects of the application are as follows:
1. the application provides a novel lead phenoxyacetate dinuclear structure complex and a preparation method thereof, and has the advantages of simple process, low cost, good repeatability, high yield and the like.
2. The application confirms that the combination mode of the synthesized novel lead phenoxyacetate dinuclear structure complex and CT-DNA is plug-in type through ultraviolet absorption spectrum, fluorescence spectrum and viscosity; the interaction between the synthesized novel lead phenoxyacetate dinuclear structure complex and HSA is verified by ultraviolet absorption spectrum and fluorescence spectrum, and the fluorescence quenching of the complex to the HSA is static quenching.
Drawings
FIG. 1 is a block diagram of a complex of the present application;
FIG. 2 is a diagram of an embodiment of the complex of the present application;
FIG. 3 is a graph showing the ultraviolet absorption spectrum of interaction of the complex synthesized by the present application with calf thymus DNA (CT-DNA).
FIG. 4 is a fluorescence spectrum of interaction of the complex synthesized according to the present application with calf thymus DNA (CT-DNA).
FIG. 5 is a graph showing the viscosity change of CT-DNA after the complex synthesized by the present application acts on calf thymus DNA (CT-DNA).
FIG. 6 is a graph showing the ultraviolet absorption spectrum of the interaction of the complex synthesized by the present application with Human Serum Albumin (HSA).
FIG. 7 is a fluorescence spectrum of interaction of the complex synthesized according to the present application with Human Serum Albumin (HSA).
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, steps, operations, devices, components, and/or groups thereof.
In order to obtain more complexes with higher activity, the present application has been studied and verified to provide the following complexes.
In a typical embodiment of the present application, a novel lead phenoxyacetate dinuclear structure complex is provided.
The molecular formula of the novel lead phenoxyacetate binuclear structure complex is C 104 H 88 N 8 O 24 Pb 4 The molecular weight is 2662.58. The complex belongs toTriclinic, P-1 space group, unit cell parameters a= 12.8054 (19) nm, b= 13.1421 (19) nm, c= 17.084 (3) nm; α= 69.914 (2) °, β= 69.972 (2) °, γ= 85.241 (2) °.
The application also provides an embodiment of the preparation method of the novel lead phenoxyacetate dinuclear structure complex, which comprises the following steps: respectively dissolving phenoxyacetic acid, 2 '-bipyridine and lead acetate trihydrate in a solvent, dropwise adding a lead acetate solution into the phenoxyacetic acid solution under stirring, dropwise adding the 2,2' -bipyridine solution into a mixed solution under stirring, regulating the pH value with a NaOH solution, filtering, and standing at room temperature for a period of time to separate colorless transparent blocky crystals.
In order to allow the ligand starting material to react sufficiently and obtain the target complex, it is preferable that the molar ratio of phenoxyacetic acid, 2' -bipyridine and lead acetate trihydrate is 1:0.8-1.2:0.8-1.2.
In the present application, the concentration of the NaOH solution is preferably 1.0 to 2.0mol/L.
In the present application, preferably, the pH is 6.0 to 6.5, and the standing time at room temperature is 10 to 15 days.
In the present application, preferably, the solvent is ethanol and ethanol-water mixed solvent.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
1. Preparation example
Example 1
Synthesis of the complex: phenoxyacetic acid (0.50 mol), 2 '-bipyridine (0.40 mol) and lead acetate trihydrate (0.40 mol) are respectively dissolved in ethanol-water solution (water: ethanol volume ratio=1:3), lead acetate solution is dropwise added into the phenoxyacetic acid solution under stirring, then the 2,2' -bipyridine solution is dropwise added into the mixed solution under stirring at the speed of 1.5mL/min, the pH value of the mixed solution is regulated to be 6.0 by 1.0mol/L NaOH solution, the solution is light milky white, filtered and kept stand for 10 days at room temperature, colorless transparent blocky crystals are separated out, and the yield is 81.4%.
Example 2
Synthesis of the complex: phenoxyacetic acid (0.50 mol), 2 '-bipyridine (0.50 mol) and lead acetate trihydrate (0.50 mol) are respectively dissolved in ethanol-water solution (water: ethanol volume ratio=1:3), lead acetate solution is dropwise added into the phenoxyacetic acid solution under stirring, then the 2,2' -bipyridine solution is dropwise added into the mixed solution under stirring at the speed of 1.5mL/min, the pH value of the mixed solution is regulated to be 6.2 by 1.5mol/L NaOH solution, the solution is light milky white, filtered and stood at room temperature for 13 days to separate colorless transparent blocky crystals, and the yield is 82.1%.
Example 3
Synthesis of the complex: phenoxyacetic acid (0.50 mol), 2 '-bipyridine (0.60 mol) and lead acetate trihydrate (0.60 mol) are respectively dissolved in ethanol-water solution (water: ethanol volume ratio=1:3), lead acetate solution is dropwise added into the phenoxyacetic acid solution under stirring, then the 2,2' -bipyridine solution is dropwise added into the mixed solution under stirring at the speed of 1.5mL/min, 2.0mol/L NaOH solution is used for regulating pH value to be=6.5, the solution is light milky white, filtered and stands for 15 days at room temperature to separate colorless transparent blocky crystals, and the yield is 81.8%.
2. Confirmation of Complex
Single crystal XRD testing was performed on the colorless transparent bulk crystals prepared in examples 1-3, and Complex [ C ] 104 H 88 N 8 O 24 Pb 4 ]The data of the crystallography, the principal bond length and bond angle, the principal twist angle, etc. are shown in tables 1, 2, and 3, respectively.
Table 1 Crystal data of the complexes
TABLE 2 principal bond lengths and bond angles of the complexes
TABLE 3 principal torsion angles of complexes
3. Investigation of Complex interactions with DNA
The complex of the application is used for researching the interaction capability of the complex and DNA, and calf thymus DNA (CT-DNA) is used as a research object.
1. The novel lead phenoxyacetate dinuclear structure complex synthesized by the application has ultraviolet absorption spectrum under the action of CT-DNA:
after baseline correction was performed by adding 2.5mL of buffer solution (Tris-HCl/NaCl) to each of the blank cell and the sample cell, the sample cell was changed to an equal volume of complex solution (5. Mu. Mol/L), an electron absorption spectrum in a wavelength range of 200 to 450nm was scanned, then 80. Mu.L of CT-DNA solution (2 mmol/L) was added to each of the blank cell and the sample cell by a pipette, and after each drop, the mixture was stirred uniformly and allowed to stand for 5 minutes, followed by scanning. FIG. 3 is a graph showing the ultraviolet absorption spectrum of interaction between the novel lead phenoxyacetate dinuclear structural metal complex of synthetic example 2 of the present application and calf thymus DNA (CT-DNA). It can be seen that the complex has a weak subtractive color at 275nm and a slight red shift in the absorption peak position as the concentration of CT-DNA increases, and thus it is presumed that the complex has an intercalating effect on CT-DNA. Calculating the binding constant K of the complex and DNA b ＝1.430×10 3 L·mol -1 。
2. Fluorescent spectrum of the action of the novel lead phenoxyacetate dinuclear structure complex and CT-DNA synthesized by the application:
ethidium bromide (EB, 8. Mu. Mol.L) -1 ) With CT-DNA solution (10. Mu. Mol.L) -1 ) Mixing uniformly with the same volume, and reacting for 12 hours. 2.5mL of EB-CT-DNA mixed solution is added into a sample cell, and the excitation is carried out at 565nm and the scanning speed is 240 nm s -1 The emission spectrum in the wavelength range of 540 to 700nm was measured. 60 mu L of complex solution is dripped into the EB-CT-DNA system(1mmol·L -1 ) After 5min of reaction, the emission spectrum was measured. FIG. 4 is a fluorescence spectrum showing interaction between the novel lead phenoxyacetate dinuclear structure metal complex of synthetic example 2 of the present application and calf thymus DNA (CT-DNA). It can be seen that the maximum emission wavelength fluorescence intensity gradually decreases as the concentration of the complex increases. At different r= [ complete ]]/[DNA]At this value, the initial fluorescence intensity was reduced from 97.80% to 72.86%. The complex and CT-DNA function mode is similar to EB and is classical insertion mode. Obtaining a quenching rate constant K q ＝2.04×10 11 L·mol -1 ·s -1 . Fluorescence quenching of EB-DNA by the complex is static quenching, binding site n=1.
3. Influence of the novel lead phenoxyacetate dinuclear structure complex synthesized by the application on CT-DNA viscosity:
the reaction temperature was controlled at 29.0.+ -. 0.1 ℃ with a constant temperature water tank, CT-DNA solution was added to the Ubbelohde viscometer, the concentration of the Complex solution was gradually increased, the concentration ratio of Complex to CT-DNA [ Complex ]/[ DNA ] =0, 0.05, 0.10, 0.15, 0.20, 0.25, 0.30 was made, and the time(s) for the CT-DNA solution to flow through the effective scale of the capillary was recorded in order, and each set of experiments was repeated 3 times, and the average was taken. FIG. 5 is a graph showing the viscosity change of calf thymus DNA (CT-DNA) after the novel lead phenoxyacetate dinuclear structure complex synthesized in example 2 of the present application reacts with CT-DNA. It can be seen that as the concentration of the complex increases, the viscosity of the DNA increases, indicating that the complex binds to the DNA in an intercalating manner.
4. Research on interaction between novel lead phenoxyacetate dinuclear structure complex and HSA
1. Ultraviolet absorption spectrum of the complex synthesized by the application and HSA:
3mL of HSA solution (200. Mu. Mol/L) was added to the sample cell, and the same amount of Tris-HCl/NaCl buffer solution was added to the reference cell, and the UV spectrum at 190-400 nm was measured. To each of the two wells, 10. Mu.L of the complex solution (0.2 mmol/L) was added, and after each addition, the mixture was blown and mixed uniformly, and after leaving at room temperature for 5 minutes, the mixture was subjected to scanning measurement in the same wavelength range. FIG. 6 is a graph showing the ultraviolet absorption spectrum of the interaction of HSA with the complex synthesized in example 2 of the present application. It can be seen that as the concentration of the complex increases, the absorption peak at 215nm has a subtractive color effect and the absorption peak position has a red shift, indicating that the complex interacts with HSA.
2. Fluorescence spectrum of the complex synthesized by the application and HSA action:
3mL of HSA solution (150. Mu. Mol/L) was added to the sample cell, and the fluorescence spectrum at a wavelength of 300 to 500 nm was measured at an excitation wavelength of 280 nm. Then 10. Mu.L of the complex solution (0.2. Mu. Mol/L) was added to the sample cell, after each addition was completed, the mixture was blown and mixed uniformly, and after 5 minutes of standing at room temperature, the mixture was scanned under the same conditions. FIG. 7 is a fluorescence spectrum of interaction of HSA with the complex synthesized in example 2 of the present application. It can be seen that HSA decreases in absorption intensity at 310nm, the strong absorption peak, as the concentration of the complex increases. Constant value K of quenching rate q ＝9.485×10 16 L·mol -1 ·s -1 Fluorescence quenching of the complex to HSA is static quenching, binding site number n=1.
The foregoing description is directed to the preferred embodiments of the present application, but the embodiments are not intended to limit the scope of the application, and all equivalent changes or modifications made under the technical spirit of the present application should be construed to fall within the scope of the present application.
Claims (5)
1. A novel lead phenoxyacetate dinuclear structure complex is characterized in that the molecular formula of the complex is C 104 H 88 N 8 O 24 Pb 4 The molecular weight is 2662.58. The data of complex crystal structure parameters, main bond length and bond angle, main torsion angle, etc. are listed in tables 1, 2, 3,
table 1 Crystal data of the complexes
TABLE 2 principal bond lengths and bond angles of the complexes
TABLE 3 principal torsion angles of complexes
2. The preparation method of the novel lead phenoxyacetate dinuclear structure complex as claimed in claim 1, which is characterized by comprising the following steps: respectively dissolving phenoxyacetic acid, 2 '-bipyridine and lead acetate trihydrate in a solvent, dropwise adding a lead acetate solution into the phenoxyacetic acid solution under stirring, dropwise adding the 2,2' -bipyridine solution into a mixed solution under stirring, regulating the pH value with a NaOH solution, filtering, and standing at room temperature for a period of time to separate colorless transparent blocky crystals.
3. The method for preparing the novel lead phenoxyacetate dinuclear structure complex according to claim 2, wherein the molar ratio of the phenoxyacetic acid to the 2,2' -bipyridine to the lead acetate trihydrate is 1:0.8-1.2:0.8-1.2.
4. The method for preparing a novel lead phenoxyacetate dinuclear structure complex according to claim 2, wherein the pH is 6.0 to 6.5.
5. The method for preparing a novel lead phenoxyacetate dinuclear structure complex according to claim 2, wherein the standing time at room temperature is 10-15 days.
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| Title |
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| L. Li et al..Hydrothermal Synthesis, Crystal Structure of Five Novel Complexes Based on 4-Chlorophenyloxyacetic Acid.《Mol. Cryst. Liq. Cryst.》.2013,第575卷(第575期),173-187. * |
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